Dislocation site density techniques

ABSTRACT

A method includes operating a gas loading system with a source of one or more isotopes of hydrogen, a gas loading chamber containing a number of metallic nanoparticles, the metallic nanoparticles being selected to provide for a predetermined hydrogen cluster formation density, a vacuum system, and a valve system in communication with the gas loading chamber, the source of one or more isotopes of hydrogen and the vacuum system; providing the gas loading chamber with a first quantity of the one or more isotopes of hydrogen from the source of one or more isotopes of hydrogen; monitoring an operating temperature; and cycling a loading pressure of the gas loading chamber using the source of one or more isotopes of hydrogen in response to providing the gas loading chamber and monitoring the operating temperature.

CROSS-REFERENCE TO RELATED APPLICATIONS

The present application is a continuation-in-part of U.S. patentapplication Ser. No. 12/080,011 filed Mar. 31, 2008, now U.S. Pat. No.8,227,020 which claims the benefit of U.S. Provisional PatentApplication No. 60/920,659 filed Mar. 29, 2007, each of which is herebyincorporated by reference in its entirety.

BACKGROUND

The present invention relates to dislocation site density techniques,and more particularly, but not exclusively, relates to dislocation sitedensity along the surfaces and formation of voids created in packed bedsof a nanoparticle structure. A variety of experiments indicate desirableproperties resulting from dislocation site density in certain materials.Standard nanoparticle production techniques provide a relatively lowdensity of such sites, which hampers the ability to prepare commerciallyviable products of interest here. Advances in production technologies tomake more active nanoparticles are disclosed.

SUMMARY

One embodiment of the present invention is a unique dislocation sitedensity technique. Other embodiments include unique methods, processes,apparatus, devices, and systems involving dislocation site density invarious thin-film and nanoparticle materials to provide for loadingdense structures of one or more isotopes of hydrogen therein. Furtherembodiments, forms, features, aspects, benefits, and advantages of thepresent application shall become apparent from the description andfigures provided herewith.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a partial schematic view of a multilayer thin film structure.

FIG. 1 a is a unique integrated thin film plate type electrode.

FIG. 1 b is a graphical representation of a heat measurement for a twolayer electrode of Palladium and Nickel thin film on alumina.

FIG. 1 c is an illustration of PdO—Pd—PdO type electrode.

FIG. 2 is a schematic view of a dislocation core formed in a lattice ofthe device of FIG. 1.

FIG. 3 is a schematic partial view of an interface between layers of theFIG. 1 device along which dislocation cores have been formed.

FIG. 4 is a flow chart describing one procedure for forming dislocationcores along the interface illustrated in FIG. 3.

FIG. 4 a is a graphical representation of temperature programmeddesorption measurements of a cluster loaded electrode shown in FIG. 1 c.

FIG. 5 is a partial schematic view of a multilayer thin film deviceincluding a void-inducing material structured to form dislocation coresalong an interface between different layers.

FIG. 6 is a computer-generated image of a micro-nickel mesh utilized asthe void-inducing material for the device of FIG. 5.

FIG. 7 is a schematic view of a multilayer thin film device includingchannels formed in one of the layers along the interface between thelayers to form dislocation cores.

FIG. 8 is a partial schematic sectional view of a device for a powersystem incorporating a multilayer thin film electrode.

FIG. 9 is a further view of the device taken along section line 9-9 inFIG. 8.

FIG. 10 is a partial schematic view of a multilayer thin film devicestructured as an inertial confinement fusion target.

FIG. 10 a is a schematic view of Petawatt laser irradiation of acluster-containing converter foil to direct MeV proton or deuteron beamsfrom the clusters onto an inertial confinement fusion target.

FIG. 11 is a schematic view of a gas loading system.

FIG. 12 is a cross section of a packed bed of nanoparticles.

FIG. 12 a is a cross section of a gas cluster formed in a void betweennanoparticles in FIG. 12.

FIG. 12 b illustrates a gas cluster formed in nano-scale pores and voidsformed in an individual nanoparticle.

FIG. 13 is a schematic with a cut-away view of a nanoparticle structure.

FIG. 14 is a graphical representation of a data set from apressurizing-depressurizing gas loading system.

FIG. 15 a is a graphical representation of a data set of a long run(temperature versus time) of a gas loading system.

FIG. 15 b is a schematic representation of a data set from a periodicdepressurizing-pressurizing gas loading system.

DESCRIPTION OF REPRESENTATIVE EMBODIMENTS

For the purposes of promoting an understanding of the principles of theinvention, reference will now be made to the embodiments illustrated inthe drawings and specific language will be used to describe the same. Itwill nevertheless be understood that no limitation of the scope of theinvention is thereby intended. Any alterations and further modificationsin the described embodiments, and any further applications of theprinciples of the invention as described herein are contemplated aswould normally occur to one skilled in the art to which the inventionrelates.

One embodiment of the present application relates to generation of ahigh density of clusters of one or more isotopes of hydrogen. In oneform, these clusters form in voids between a bed of packed nanoparticlesand at interfaces of multi-layer thin film structures. In another form,the clusters form along the surfaces of nanoparticle structures. In oneexample of the multilayer structure, stress-created dislocation defectssuitable for the formation of such clusters are created at theinterfaces between thin films by cyclic loading and deloading ofhydrogen. Alternatively or additionally, a further form employsplacement of nanoscale particles or fibers between the interfaces tocause suitable void sites during manufacture of the films. Otherembodiments include configurations of the structures for use insuperconductors, charged particle and/or x-ray sources, and/or for usein power systems.

A further embodiment is illustrated as multilayer thin film device 20 inFIG. 1. Device 20 includes two multilayer thin film stacks 26 onopposite sides of base/substrate 24. Each stack 26 includes alternatinginner layers 28 of different types of metals designated as palladium(Pd) and nickel (Ni), respectively. Between each inner layer 28 of Pdand Ni, a Pd/Ni interface 30 is formed, only a few of which arespecifically designated to preserve clarity. In one form, the base 24 isfabricated from stainless steel or aluminum; however, other materialsmay be used in different embodiments.

In one alternative embodiment, the alternating inner layers 28 are oftwo dissimilar metallic materials. In a further embodiment, thealternating layers 28 are a metal and an oxide of metal, such asalternating inner layers of Pd and PdO. In another form, one layer 28for each interface 30 is comprised of a material that readily forms ahydride and the other layer 28 for such interface 30 is comprised ofmaterial in which isotopes of hydrogen are readily accepted. By way ofnon-limiting example, Pd and Ti readily form hydrides and Ni readilyaccepts hydrogen loading. In still another form, one of the alternatinginner layers 28 includes one element selected from a group consisting ofPd, Ti, Ni, Li, Au, Ag, U, and alloys thereof, and the other of thealternating inner layers 28 includes a different one of this group. Thisform is intended to include alternating layers each comprised of adifferent alloy of Pd, Ti, Ni, Li, Au, Ag, and/or U.

For embodiments utilizing a continuous reaction, a flux of ionsdiffusing through the multilayer structure may be maintained. Oneembodiment is designed for hydrogen isotopes in an electrolysis unit toaccomplish this as shown in FIG. 1 a. In this embodiment a multilayertype structure of FIG. 1 is located on a non-electrical conductingsubstrate 110 a such as but not limited to quartz. The layer structureis shown coated with a diffusion barrier 120 a such as chromium, forexample, on a top surface 121 a and a side surface 122 a. An electricalconnection 150 a from the electrodes is connected to an electrolysispower supply such that an electronic field is created from an anode 130a to a cathode 140 a parallel to substrate 110 a. The well boronelectromigration effect forces the hydrogen isotopes to enter andtransport through cathode 140 a of thin film 101 a parallel to substrate110 a. Film interfaces provide volumetric loading and local clusterformations due to the corresponding ion hydrogen formation and acontinuous ion flux in the same direction. The degree of loading and thenumbers of clusters can be controlled by constructing the area of theexit region smaller than the entrance region by partially covering theexit surface with diffusion barrier 120 a such as used on the top andsides of the multi-layer structure. Formation of a smaller area sectionfor exiting hydrogen isotopes reduces the exit flow causing a build-upin density of isotopes in this region which in turn results in thehigher loading there.

This embodiment of creating an ion flux also allows an increase (ordecrease) in reaction rates in the multilayer electrode. One specificembodiment includes pulsing an applied voltage between a set ofelectrodes by an external power supply. The resulting change in theinduced electrical field created parallel to a substrate in turn changesthe ion flux driven by electromigration. The effect of stepping thevoltage up and down and the corresponding change in reaction rate, andhence power output of the electrolysis cell placed in a calorimeter, isillustrated in FIG. 1 b. After each rapid increase (or decrease) involtage, the percentage of power increase above that caused by theelectrified input for electrolysis increases (or decreases), whichindicates a corresponding change in reaction rate. Other embodimentssuch as but not limited to the application of laser light, ultrasound,radiofrequency waves, etc., may be used to change the ion diffusion rateor flux. These embodiments may then serve as a method to adjust orcontrol reaction rates in electrolytic apparatus employing multilayerthin film electrodes. In yet another embodiment illustrated in FIG. 1 c,a thin Pd film 121 c or layer is formed between PdO layers 120 c formedby heating the Pd surface in an oxygen environment. This embodimentrepresents a three layer configuration, the central layer 121 c beingunconverted Pd. For some applications, a supporting substrate couldsubstitute for the lower PdO film. This embodiment is particularlyuseful in situations where electron, ion, or laser light is directed atthe Pd-based object after loading with a hydrogen isotope and clustersformed by the loading-deloading technique described herein. In one suchembodiment, irradiation with a pulsed Petawatt laser drives the hydrogenisotope ions out of the cluster filled film forming energetic particlebeams.

Referring to FIG. 2, schematically shown is an atomic lattice 40 with arepresentative dislocation core 42 formed along interface 30 in aportion 44 of two internal layers 28 of device 20 in FIG. 1 (not toscale). A number of hydrogen atoms comprise cluster 46 in core 42, whichmay be comprised of one or more hydrogen isotopes (¹H, ²H or D(deuterium), ³H or T (tritium)). In one form, dislocation core 42 isstructured to receive a cluster 46 of at least 5 hydrogen atoms orisotopes thereof. In a more preferred form, dislocation core 42 isstructured to receive a cluster 46 of at least 50 hydrogen atoms orisotopes thereof. In an even more preferred form, the dislocation core42 is structured to receive a cluster 46 of at least 500 hydrogen atomsor isotopes thereof.

Referring additionally to FIG. 3, a number of dislocation cores 42 areshown schematically along interface 30 formed between inner layer 28 ofPd and inner layer 28 of Ni for device 20. In FIG. 3, the Pd layer ismore specifically designated by reference numeral 62 and the Ni layer ismore specifically designated by reference numeral 64. It should beunderstood that the nature of Pd as a more favorable hydride formingsubstance than Ni likely results in the formation of dislocation cores42 in layer 62 at interface 30. The dislocation cores 42 containmismatched atomic structures due to the different materials on each sideof the interface 30—making it susceptible to stress-createddislocations, such that a large density of dislocation sites for clusterformation can be obtained with some degree of uniformity along thesurface area of interface 30. The use of multiple thin film layers withmany interfaces 30 approximates a nearly uniform three-dimensionalvolume for dislocation (and correspondingly cluster) sites to form.

In one embodiment, a technique to increase formation of dislocationcores involves preparing the thin film layer interface 30 using one ormore different procedures. In one non-limiting form, a predefined targetrepresentative of a desired dislocation site density of a multilayerthin film device design is established, and a multilayer thin filmdevice is formed according to the design. This device formation includesproviding a first layer of a first type of material and a second layerof a second type of material dissimilar from the first type of materialand preparing an interface between the first layer and the second layerto increase a quantity of dislocation sites there along incorrespondence with the predefined target. After forming, the multilayerthin film device is supplied with one or more isotopes of hydrogen toform hydrogen clusters in the dislocation sites to facilitateapplication as a superconductor, an X-ray source, a charged-particlesource, as a power supply component, or the like.

FIG. 4 provides a flowchart of one non-limiting procedure 220 of thepresent application to promote dislocation core formation. Procedure 220begins with providing a thin film structure, such as device 20 inoperation 222. Procedure 220 continues with operation 224 in which thethin film structure is loaded with one or more isotopes of hydrogenusing any of several techniques. These techniques include: electrolysishydrogen loading, pulsed plasma bombardment hydrogen loading, and gaspressure hydrogen loading. During loading, the metal lattice is expandedby the entering hydrogen atoms, creating stress which causes dislocationcore formation. In one implementation, loading occurs at severalatmospheres for several hours. After loading, the structure is deloadedin operation 224. Deloading of the loaded hydrogen allows repetition ofthe loading stresses and progressively forms added dislocation cores. Insome embodiments, the deloading process may include features such asheating the system to several hundred degrees C. for times up to 2-3 hrsto remove volumetric hydrogen. In other embodiments, a deloading processmay not include such features when clusters operate at >600° C.

In one non-limiting form, deloading occurs for about two hours bypumping a chamber containing the structure down to hard vacuum. Therelative volumetric loading and cluster loading can be tested using avacuum oven which can slowly heat a sample film up to high temperatures.Illustrated in FIG. 4 a, as the sample film heats up in the vacuum oven,the hydrogen gas pressure in the oven chamber increases (measured with agas analyzer to eliminate contaminate gas such as but not limitednitrogen, oxygen, etc., from adding to the pressure recorded). Theinitial build up comes from volumetric hydrogen but at highertemperatures (around 450 and 800° C.) peaks in pressure occur due to arelease of the more tightly bound hydrogen (or deuterium) clusters. Twopeaks are observed in the data shown in FIG. 4 a and can be attributedto smaller less dense more weakly bound clusters followed by the largerpeak attributed to the more strongly bound, more dense cluster hydrogenin an ultra dense cluster.

From the loading/deloading of operation 224, procedure 220 continueswith conditional 226. Conditional 226 tests whether a desired level ofdislocation core formation has taken place. If the test outcome is false(no), then the loading/deloading cycle of operation 224 is repeateduntil the test is true (yes). The cycle may be repeated for several daysup to a week or more, and such cycles may be timed and or with othersalient parameters that are uniform/periodic from one to the next ornon-uniform/aperiodic in nature. In one form, at least 5 cycles areperformed. In a more preferred form, at least 10 cycles are preformed.In some cases it may be necessary to perform at least 25 cycles.

Returning to FIG. 4, the test may be satisfied simply when apredetermined number of loading/deloading cycles of operation 224 arecompleted. Alternatively or additionally, the test of conditional 226may be satisfied by direct observation and/or by indirect measurement.In one example, the test is satisfied by gas pressure measurements todetermine flows in and out of the sample during loading and deloading.The process is continued until these pressure measurements indicate thata saturation amount of retained gas is achieved, i.e. a maximum numberof target dislocation site/clusters has been formed. From conditional226, procedure 220 continues with operation 228. In operation 228,hydrogen is supplied to the structure to provide clustering in thedislocation cores formed by the repetitive loading/deloading cycles andapplied as desired as a superconductor device or cable, an X-ray source,a charged particle source, as a power supply component, or the like. Inanother embodiment, volumetric loading may be selectively removed(leaving only hydrogen in cluster sites) by low temperature (≲300° C.)desorption as was done in the cycles of 224. Following such a procedure,operation 228 may incorporate a hydrogen isotope loaded structure withmultiple plates into a cell. Such a cell may involve creation of asuperconductor device or cable, an X-ray source, a charged particlesource, as a power supply component, or the like. Depending on theapplication, a continuous flow of one or more hydrogen isotopes may beprovided in operation 228 and/or an intermittent supply provided.

A further procedure for forming dislocation sites at the thin filminterfaces involves placing microscale and/or nanoscale material betweenthe layers. This material is in the form of particles, wires, fibers,meshes, a porous film/layer, or a combination of these. FIG. 5schematically illustrates thin film device 320. Device 320 includes thinfilm layer 322 and thin film layer 326 with a dislocation site-inducingstructure 324 positioned there along the resulting thin film layerinterface 330. Structure 324 can be a microscale and/or nanoscalematerial that causes voids and discontinuities to form along theinterface in the nanoscale range. It should be appreciated thatmicroscale materials frequently are structured to form nanoscale voidsbetween its constituents and/or with one or more of layers 324 and 326,from which dislocation cores result. Specifically, the thickness of thestructure involved is desirably selected to obtain the dislocation sitedensity. Generally, dislocation sites form around the intersections ofthe microscale/nanoscale structures where a higher density of voidspaces can occur between layers. Note that with preformed nanoscalevoids in the structure 324, loading without cycling can achieve a higherdislocation site and corresponding hydrogen isotope cluster density.

FIG. 6 illustrates a computer-generated image of a micro-nickel fiber(MNF) mesh 424. Mesh 424 is one non-limiting form of structure 324. Mesh424 has dimensions in the microscale range as can be observed in theimage of FIG. 7, which includes a reference distance of 100 micrometers(100 μm) in the bottom center portion. In one process that used MNF, aPd film is sputtered onto a ceramic substrate, and the MNF is thenplaced on top of the Pd film. This arrangement is then heated andmaintained at several hundred degrees C. in a vacuum chamber for ˜2hours for out-gassing and annealing. Next, a second thin film issputtered onto the top of the MNF. The process is then repeated tobuild-up the desired layering for the multilayer device. FIG. 7illustrates multilayer thin film device 520 that incorporates anothertechnique to provide for the formation of nanoscale voids that inducedislocation site formation. Device 520 is partially shown, includingthin film layer 524 and thin film layer 526 that form interface 530there. Along interface 530, a number of microscale and/or or nanoscalechannels 528 are formed in the face of layer 524 to provide for theformation of dislocation sites. In one form, micro-grooving is used tocreate a “scratch” pattern on the thin-film prior to deposition of thesubsequent layer. While sputtering was used in these preparations, inother embodiments alternate techniques can be used, such as plasmadeposition, electroplating could be used, chemical vapor deposition,and/or or physical vapor deposition could be used.

While only shown with two layers, it should be understood that device320 or 520 can each include a greater number of alternating thin filmlayers to provide a number of interfaces 330 or 530 between eachalternating layer pair. It should be appreciated that the alternatelayer compositions described in connection with device 20 can also beutilized with device 320 and/or device 520. Likewise, it should beappreciated that any of the dislocation core formation techniques (andcorrespondingly the cluster formation techniques) described with anyembodiment of these devices can be used in combination or asalternatives to one another in other embodiments. It should beunderstood that when multilayers are used, the unused unreactivematerial interface can be minimized to increase the volume percentageoccupied by voids and/or dislocations where clusters are formed.

A number of different implementations of the thin film structures of thepresent application are envisioned. For instance, FIGS. 8 and 9 depict ahydride-loaded, thin-film multilayer electrode power system 620. FIG. 9is taken along section line 9-9 of FIG. 8, illustrating an approximatelycylindrical profile. System 620 includes a multilayer thin filmelectrode structure 624 inside a cylindrical housing 622. Structure 624includes alternating inner layers of Pd and Ni, with an outer barrierlayer of a non-diffusing material such as chromium or platinum and aninner platinum (Pt) block 627 covering the inner portion of the thinfilms. Inner Pt block 627 may be situated such that diffusing hydrogenisotope ions enter the larger portion of the uncovered thin film layers,diffuse parallel to the films and exit on the smaller uncovered portionof the thin films. This configuration is equivalent to the design shownin FIG. 1 a.

Inside structure 624 is a hydride donor layer 626 structured to donateprotons, such as (LaNiH_(x)) for cluster formation in dislocation sitesof structure 624. Inside layer 626 is a semitransparent oxide layer 628.A standard-type thermoelectric converter layer 625 is included outsideof structure 624 to convert thermal energy from the electrode toelectrical energy. Radial fins 630 provide for thermal dissipation inconcert with coolant flow (such as ambient air) represented by arrow640. U.S. Pat. No. 7,244,887 (issued Jul. 17, 2007) provides additionalbackground information regarding this type of power system arrangement,and is hereby incorporated by reference.

The Pd and Ni films of structure 624 are prepared on a cylindricallyshaped Pt substrate block using one or more of the techniques to prepareenhanced dislocation site density and corresponding cluster formation,as described in connection with FIGS. 1-7. Structure 624 could usedifferent thin film compositions, layer quantities, and the like of anyof the embodiments previously described in connection with FIGS. 1-7.

Another application of any of these embodiments is to providesuperconducting structures. Such structures could be in the form of thinplates or in the form of wires. In one non-limiting superconductorimplementation, thin film structure geometry is selected to formdislocation cores that provide a corresponding hydrogen cluster densitywith a large cross sectional area. As previously described, still otherembodiments utilize the inventive aspects of the present application toprepare multilayer thin film structures for X-ray and/or high energy(MeV) charged particle sources. Emission of both energy forms has beenobserved for Ni/Pd thin-film structures, but other combinations ofmaterials may be selected.

The principles described here for plate type thin film can be extendedto other geometries, such as rods or spheres. The geometry employment isoften driven by the intended application. For example, in a particularembodiment, hydrogen isotope storage could use plate geometry; inanother embodiment, hydrogen isotope storage for a superconductive“cable” could use rods. Another specific embodiment includes internalconfinement fusion (ICF) which can use a spherical arrangement.

FIG. 10 depicts a small spherical inertial confinement fusion target 700of yet a further embodiment of the present application in a partialschematic, cutaway form. In one non-limiting form, target 700 is anapproximately spherical, ultra-high density inertial confinement fusionfuel (ICF) target and is provided in the micron to millimeter sizerange. A conventional ablator-tamper 701 (such as described in S. Atzeniand T. Meyer-TerVehn, The Physics of Inertial Fusion, Oxford UniversityPress, 2004, which is hereby incorporated by reference), surrounds amulti-layer device 702. Device 702 includes alternating layers ofdifferent materials with interfaces suitably forming a region ofdislocation cores prepared according to one or more of the previouslydescribed embodiments of the present application. Low atomic number Zmaterial selection, such as but not limited to Beryllium and Lithium ispreferred to avoid excessive Bremsstrahlung emission during laserinteraction and compression. The dislocation cores of this region areloaded with hydrogen isotopes such as deuterium and/or tritium. Whenexposed to a pulsed laser beam or ion beam of sufficient intensity (suchas available at the ICF facility at the Lawrence Livermore NationalLaboratory (USA)), ablation of the ablation-tamper 701 material resultsin compression of the core region 702—such compression may be by afactor of 100 to 1000 in terms of volume. Because the hydrogen isotopeclusters in dislocation sites start at densities typically well abovethat of gaseous or cryogenic deuterium-tritium generally employed, thecompressed density of the isotopes in the clusters will becorrespondingly higher, which in turn can result in higher fusion rates(proportional to the square of the isotope density) and an increasedburn-up fraction (fraction of the original isotope burned in theimploded target). This improved performance is of interest for fusionpower studies and applications thereof (such as power systems),particle/radiation generation, and the like. Additionally oralternatively, target 700 can be adapted to other types of targetscurrently employed in ICF studies such as indirect-drive holrahm targetsas further described by Atzeni and Meyer-TerVehn in The Physics ofInertial Fusion, Oxford University Press, 2004, (previously incorporatedby reference).

Another embodiment for an ICF application is termed “fast ignition,”which uses Petawatt laser interaction with a deuterium cluster thin-filmfocus to produce MeV deuterium ion beams focused on an ICF sphericaltarget in order to provide the ignition of the target burn. The use ofpulses of MeV ions such as protons, deuterons, or others such as carbonhas been studied at various DOE laboratories such as LANL. Preliminaryexperiments with a cluster target at LANL have established beamformation from a cluster thin-film using a Petawatt laser. One featureincludes a high “contact ratio,” i.e., ratio of laser light intensity onthe film just prior to actual achievement of the peak pulse intensity.While other deuterium containing films can be used, the cluster filmoffers improved features such as substantially continuous availabilityof deuterium through the length of the laser pulse, better laser energyutilization as the metal host material is much heavier than deuterium,and thus has little acceleration and low sharing of laser energy withdeuterium.

A further embodiment of the present application relates to the formationof a high density of one or more isotopes of hydrogen at surfaceinterfaces of nanoparticle structures. In a specific embodiment, thepreviously discussed effect of forming layer “dislocations” may beprovided by the interstitial spacing of nanoparticles. The nanoparticlesmay create interstitial trapping zones for the hydrogen ions withnanoparticle surface topography and roughness, plus voids formed in apacked bed of nanoparticles. In another embodiment, surface adsorptionmay trap hydrogen or one of its isotopes such as but not limited todeuterium on the surfaces. The hydrogen isotope may be is dissociated.After which the hydrogen isotope may diffuse into the inner lattice ofthe nanoparticles and form volumetric loading with high densitylocalized clusters (such as described for thin films earlier).

A low energy reaction system 1100 of the present application as shown inFIG. 11 includes a gas loading system 1101, a hydrogen gas source 1120,a pressure control system 1150 and a gas loading chamber 1130 containingnanoparticles 1111 in the solid phase. Nanoparticles 1111 can be in anyform, such as a powder in the nanoscale regime, one or more structuresformed from nanoparticles or the like. Pressure control system 1150 isshown in FIG. 11 as a set of vacuum systems 1110 and a set of valves1140, 1141, 1142. Pressure control system 1150 is capable of providing aquantity of gas from hydrogen gas source 1120 to gas loading chamber1130 and producing a reaction pressure in gas loading chamber 1130. Toreduce impurity gases from entering the nanoparticle chamber in thesource gas, a cryogen temperature (e.g. liquid N₂) may be included inthe gas inlet line. One embodiment of this feature may include a coldtrap (not shown) having a chamber of cryogenic material such as liquidN₂.

Once a preset pressure is achieved, valves 1140, 1141 can be closed tomaintain the pressure and then periodically reopened for a brief time tofurther increase the pressure or to adjust for pressure reduction due toleakage or reaction consumption. Valves 1140, 1141 are capable ofdirecting a first quantity of a hydrogen isotope from a hydrogen isotopegas source 1120 into gas loading chamber 1130 under a gas loadingpressure provided by vacuum systems 1110. Valve 1142 may be operated todirect at least a portion of the hydrogen isotope gas from gas loadingchamber 1130 thereby reducing the gas loading pressure. Still further, asecond quantity of a hydrogen isotope can be loaded in gas loadingchamber 1130 under another gas loading pressure provided by vacuumsystems 1110. Gas loading system 1101 may be operable to cycle a loadingpressure of gas loading chamber 1130 using vacuum system 1110 whenproviding one or more hydrogen isotopes from hydrogen gas source 1120 togas loading chamber 1130.

A thermal management system 1160 may also be included in low energyreaction system 1100. Elements 1165 for heating and/or cooling can beused to help control temperature conditions for gas loading chamber1130. Thermal management system 1160 may provide a vacuum space forreduction of heat conductor loses. Thermal management may be applied toa gas loading system of a low energy reaction system to providetemperature control of a reaction within the system and/or temperaturecontrol of the system. Heating elements, such as but not limited tocoils, rods, radiation, microwave and the like, may be applied tocontribute to the initiation of a reaction during gas loading phases. Inanother embodiment, active cooling elements, such as plates, fins,tubes, fingers, pipes, pools and the like, may be applied to managetemperatures. Heating and cooling elements may be placed in variouspositions in the system relative to the nanoparticles to affect thermalmanagement as one skilled in the art would understand.

A gas loading system may reach temperatures capable of sintering atleast a portion of the nanoparticles together, setting an upper limitfor the temperature controller. Operation within temperature limits maybe achieved by periodic depressurizing-pressurizing steps as illustratedin FIGS. 15 a and 15 b. In one specific embodiment, thermal managementof the system may be designed to maintain the nanoparticle bed within aband of temperatures. In one particular embodiment, the maximumtemperature can be set to avoid sintering or melting of thenanoparticles in the gas loading chamber. For instance, nanoparticles inthe gas loading chamber of an embodiment of the present application mayinclude a potential for thermal variances or hot spots which maycontribute to nanoparticle sintering. High temperatures in the systemmay lead to deteriorating or sintering of the nanoparticles within thegas loading chamber and result in loss of surface area thereby affectingthe gas loading efficiencies. The sintered particles may also limit aflow of hydrogen ions from the hydrogen ion source into the gas loadingchamber which initiates or maintains a reaction.

The lowest temperature can be set such that an LENR reaction rate isself-maintained (experiments show that reactions decay if the bedtemperature is below a certain value). Operation near the uppertemperature limit is preferable because following the Carnot law forideal efficiency, the efficiency for heat conversion to electricityincreases as the difference between the maximum temperature and the heatsink temperature increases. The thermal management system may furtherinclude a temperature monitor. In one embodiment, a gas loading systemmonitors an operating temperature of the gas loading chamber andnanoparticles. The gas loading system may cycle a loading pressure ofthe gas loading chamber removing and providing one or more isotopes ofhydrogen in response to the operating temperature. However, if suddenpressure changes are employed to maintain operation, a slow decrease intemperature towards the minimum limit may result. In that instance, thesystem may maximize the time-averaged temperature during operation.

The gas loading system may include a single chamber within the system ormay constitute a variable number of chambers with various geometriespossible. Variation in the chamber design may affect thermal properties,gas flow properties, nanoparticle filling properties and the like. Inanother embodiment, a hydrogen gas source may include hydrogen ions suchas ¹H, ²H or D (deuterium), ³H or T (tritium). In yet anotherembodiment, a pressure control system may include at least one pressurevalve or a system of pressure control apparatuses to facilitate andmaintain the gas loading pressure, facilitate depressurizing the systemand facilitate alternating between pressurizing and depressurizingphases. Such valves may allow setting the rate of pressure change inthese operations.

Referring to FIG. 11, gas loading chamber 1130 includes at least apartial fill of nanoparticles 1111. The partial fill of nanoparticlesmay result in a gas reservoir under pressure related to the nanoparticlebed within the gas loading chamber, a degree of freedom in nanoparticlemovement in the gas loading chamber, and the like which may contributeto the efficiency level of the gas loading system. In other embodiments,the gas loading system may include a filter to keep nanoparticles fromescaping. This filter may include a fine-woven clothe of sufficient meshsize to prevent passage of the particles but allow gas flow with minimumpressure drop. A filter may be placed at an inlet position relative tothe gas loading chamber. A filter may also be placed at the surface ofthe nanoparticle bed inside the gas loading chamber. A substantiallyfull nanoparticle bed or a filter placed on the bed surface may becapable of affecting the efficiency of the gas loading system.

In one embodiment, gas loading of the gas loading chamber containingnanoparticles may be a triggering event for reactions. Other triggeringevents may be present, such as but not limited to pressure pulses,initial heating by exothermic chemical reactions, and external heating.Alternatively, a series of load, gas react, release and reload gasevents may be applied. When gas is loaded to the system, the increase inpressure provides an increase in temperature. The initial increase inpressure and temperature may be the catalyst for a series or group ofexothermic reactions. These exothermic reactions may contribute to afurther increase in temperature. In another embodiment, a suddendepressurization of a low energy reaction system of the presentapplication may trigger a second temperature increase instead of atemperature decrease as would be expected with a decrease in pressureunder typical operating conditions. FIG. 14 is a graph of arepresentative data set showing the temperature increase after gasloading has started, a somewhat steady-state phase and anothertemperature rise when unloading starts. The sudden depressurization maybe provided through the pressure control system.

During the adsorption of the hydrogen ions by the nanoparticles whilegas loading under pressure in the gas loading system, an exothermicreaction may take place. The chemical reaction energy may be expressedas:Chemical Reaction Energy=ΔH×M _(D2)

ΔH=−35,100 J per mole of D₂ for the formation of PdD_(x) for x<0.6;

M_(D2) is the total moles of D₂ that combined with Pd.

Consequently, the total energy (chemical+nuclear) calculation may beexpressed as:Total energy=ΔT(M _(chamber) S _(chamber) +M _(powder) S _(powder) +M_(gas) S _(gas))where ΔT is temperature change, M is mass and S is specific heat.Chamber subscripts indicate the total chamber values, powder subscriptsrepresent the nanoparticles contained therein, and gas subscriptsrepresent the gas contained in the chamber. The total heating energy maybe calculated by considering the heat capacity of both the gas loadingchamber and the nanoparticle powder loaded into it.

In another embodiment, the efficiency of a reaction within the gasloading system may be in relation to the cluster loading plus the flowor flux of hydrogen ions into or through the nanoparticles. This isanalogous to the loading and ion flow or flux effect for thin film plategeometry structures illustrated earlier in FIGS. 1, 1 a and 1 c. Ionflow may provide reactant interactions by transfer of energy andmomentum to cluster atoms, keep the system from becoming stagnant, andthe like. After gas loads a gas-loading chamber, the flow of ions in thenanoparticles continues but decreases as the loading reaches a maximumvalue. Following which the flow occurs to replace reacted isotopes andto fill new voids that may be created in the particles. A suddendepressurization may trigger a flow of ions with an internal pressurecapable of forcing a more efficient flow.

In yet another embodiment, a process begins with gas loading a gasloading chamber of nanoparticles. As the reaction(s) are initiated andthe temperature increases, a quasi-steady-state may be reached. Alongthe reaction timetable, the temperature may begin to decrease. At apoint along the temperature curve, a sudden depressurization of the gasloading system may be provided. The depressurization may be used toreestablish the ion flow within the nanoparticles, but rather thaninward flow as during pressurization, this flow is outward as thepreviously absorbed gas is desorbed. The depressurization flow may causean increased transfer of momentum to the atoms in the yet un-reactedcluster deposits, therefore increasing the reaction rates in theseclusters. However, as the chamber pressure drops, the flow may begin todecrease since the absorbed ion density decreases, causing acorresponding decrease in temperature. At some point the chamber may bequickly re-pressurized, thus re-establishing an inward flow or flux ofions in the nano-particles. The inward flow may increase momentum flowsuch that the reaction rate and temperature again increase until theinward flux slows down as the absorption begins to saturate. However, insuch an embodiment, while the pressure is maintained, the slow drop inreaction rate that follows may be slower than the drop after a suddendepressurization where the pressure remains low during the drop period.Such a cyclic method, starting with pressurization and depressurization,then re-pressurization and re-depressurization etc. may allow long runssuch as months or years, with the temperature of the packed bed beingmaintained between a predetermined range of maximum and minimumtemperature bounds. Timing for cyclic pressurization-depressurizationmay determine the upper and lower bounds for the temperature. For anembodiment which operates as a “heat engine” (i.e. conversion of a heatsource to electrical output), the Carnot Cycle theoretical efficiencyindicates that the highest maximum temperature (while avoiding damage tothe nano-particles) and a small difference between upper and lowertemperature bounds may be determined.

Two embodiments of temperature control are illustrated schematically inFIGS. 15 a and 15 b. FIG. 15 a illustrates a cycle without temperaturecontrol. In this embodiment, the temperature rises quickly to a maximumvalue upon start up and then decays quickly while the chamber remainsdepressurized. In the embodiment shown in 15 b, cyclic pressure controlis used to maintain operation over a long period of time. In thisembodiment, an initial start-up is essentially the same as in FIG. 15 a,but after the rapid temperature fall with depressurization,re-pressurization and a corresponding temperature rise follow. Thesubsequent fall-off in temperature may be slower in response to thechamber remaining pressurized. The pressurization/depressurization cyclemay be repeated. The process described in this embodiment may be one ofseveral methods that may be applied to achieve temperature control forlong runs. Other methods may include, but are not limited to,depressurization and pressurization (reverse sequence from FIG. 15 b),and use of external factors such as ultrasound, laser radiation,external heating and external cooling. FIG. 15 b illustrates theapplication of pressurizing and depressurizing.

In another embodiment, there are several possible locations that maypromote cluster formation which may represent an ability for maximizingthe density of clusters, hence maximizing the reaction rate densities inthis configuration. Nanoparticles having hydrogen/deuterium clusterslocated in the interstitial spacing of the nanoparticles areschematically shown in FIGS. 12, 12 a, and 12 b. Under pressure and in agas loading chamber, hydrogen clusters 1220, 1230, 1240, may be formedin void spaces. Void spaces may include the interstitial space betweennanoparticles 1210 and in natural formations 1230 such as but notlimited to channels, holes and pores. Pores may be formed with neckedoff passage to the surface which may be produced by surface meltingduring heating of the nanoparticles. Further, voids 1250 (or dislocationloops) may be formed near the surface of an individual nanoparticle1210. In the schematic illustrations of FIGS. 12, 12 a and 12 b,nanoparticles are represented as spheres, but nanoparticles may have avariety of shapes. Nanoparticles 1210 may have more surface area thanthin films and thus a larger area for hydrogen clusters 1220 to locate;thereby increasing the relative density of cluster atoms 1220 innanoparticles 1210.

During operation of an embodiment of the present application, clustersmay disappear due to reactions taking place while others may be formedas new void spaces are created, representing a dynamic situation. If thenet number of unreacted clusters decreases, it may be necessary toremove the nanoparticle bed and reload the chamber with freshnanoparticles to initiate a new run. In a modified chamber design, freshparticles located in a separate chamber could be rotated in to minimizedowntime. Likewise a new gas source can be inserted as needed ormultiple sources may be incorporated into the system to allow “in place”switching.

In addition to the added surface to volume advantage, nanoparticles maybe manufactured using select sizes, select alloy materials and selectsurface roughness conditions to further increase hydrogen isotopecluster density. In one non-limiting embodiment, nanoparticles aremanufactured by grinding alloyed billets, rods, bricks and the like.Grinding may include ball milling. Preparing nanoparticle may includeprocesses such as but not limited to milling, annealing, supplementalannealing, sizing, filtering and combinations thereof. The resultingnanoparticles may include a surface area and topography including localsurface roughness which may contribute to hydrogen loading and clusterformation. Other embodiments may include nanoparticle manufacturingprocesses which produce various other surface topographies and roughnessas known in the art.

For one embodiment, a microsphere design may include layers of metalswith dissimilar Fermi levels to increase the hydrogen ion density duringgas loading. A microsphere 1300 with a sputter coating is shown in FIG.13 with a core material 1305, an intermediate layer 1304 which may be acopper flash and the like, a first metal layer 1303, a second metallayer 1302, and a repeated first metal layer 1301. In one specificembodiment, the first metal may be nickel and the second metal may bepalladium. In a variation, the microsphere design may substitute the lowZ metals in the layers.

In various embodiments, nanoparticles may include a Pd-rich compositionand a Ni-rich composition. The Pd-rich composition may be gas loadedwith high purity D₂ (or heavy water). The Ni-rich composition may be gasloaded with H₂ (or light water). The Pd-rich composition may include upto 100 weight percent palladium. The Ni-rich composition may include upto 100 weight percent nickel. Alloying elements such as but not limitedto zirconium may be included along with palladium and nickel tocontribute to the efficiency of the gas loading system by includingmetals in the alloy with dissimilar Fermi levels. Alloying compositionsmay include, for example:

35 weight percent palladium and 65 weight percent zirconium with D₂loading;

20 weight percent palladium, 15 weight percent nickel and 65 weightpercent zirconium with H₂ or D₂ loading; and

35 weight percent palladium, 15 weight percent nickel and 50 weightpercent zirconium with H₂ or D₂ loading.

One aspect of the present application is a method having the steps ofoperating a gas loading system including: a source of one or moreisotopes of hydrogen, a gas loading chamber containing a number ofmetallic nanoparticles, the nanoparticles being selected to provide fora predetermined hydrogen cluster formation density, a vacuum system, anda valve system in communication with the gas loading chamber, the sourceof one or more isotopes of hydrogen and the vacuum system; providing thegas loading chamber with a first quantity of the one or more isotopes ofhydrogen from the source of one or more isotopes of hydrogen; monitoringan operating temperature; and cycling a loading pressure of the gasloading chamber using the source of one or more isotopes of hydrogen inresponse to providing the gas loading chamber and monitoring theoperating temperature.

Features may include the metallic nanoparticles being a palladium richalloy and the first quantity of the one or more isotopes of hydrogenbeing deuterium (D₂) and where the palladium rich alloy further includesabout 35 weight percent palladium and about 65 weight percent zirconium;and the metallic nanoparticles being a nickel rich alloy to produce aquantity of nanoparticles and the first quantity of the one or moreisotopes of hydrogen further being hydrogen (H₂) and where the nickelrich alloy further includes about 20 to about 35 weight percentpalladium, about 15 weight percent nickel and about 50 to about 65weight percent zirconium. Another feature may include providing athermal management system where the thermal management system mayfurther include at least one of a heating element and a cooling element.Yet another feature may include: removing impurities with a vacuum inthe gas loading chamber containing the number of metallic nanoparticles;and desorbing a quantity of gases by heating the gas loading chambercontaining the number of metallic nanoparticles.

Another aspect of the present application is a system including a gassource to provide one or more isotopes of hydrogen; a plurality ofmetallic nanoparticles; a chamber containing the metallic nanoparticlesand structured to receive the one or more isotopes of hydrogen from thegas source; a vacuum system; a valve system in communication with thechamber, the gas source and the vacuum system where the valve system iscapable of directing a first quantity of the one or more isotopes ofhydrogen from the gas source into the chamber under a gas loadingpressure provided by the vacuum system and directing a second quantityof the one or more isotopes of hydrogen from the chamber therebyreducing the gas loading pressure.

Features of this aspect may include the valve system being capable ofdirecting a third quantity of the one or more isotopes of hydrogen fromthe gas source into the chamber under a second gas loading pressureprovided by the vacuum system and having a first valve to disconnect thevacuum system from the gas loading chamber and a second valve todisconnect the hydrogen gas source from the gas loading chamber; thenanoparticles may include a palladium alloy where the first quantity ofhydrogen includes deuterium (D₂) and where the palladium alloy mayfurther include about 35 weight percent palladium and about 65 weightpercent zirconium; the nanoparticles may include a nickel alloy wherethe first quantity of hydrogen includes hydrogen (H₂) and where thenickel alloy may further include about 20 to about 35 weight percentpalladium, about 15 weight percent nickel and about 50 to about 65weight percent zirconium.

A further feature of this aspect includes a thermal management systemwhich may include at least one of a heating element and a coolingelement. Yet another feature may include directing a quantity of initialgases from the chamber containing the nanoparticles where the thermalmanagement system is capable of modifying a temperature of the chambercontaining the nanoparticles during directing the quantity of initialgases.

Yet another aspect of the present application is a method including thesteps of providing several nanoparticles each comprised of at least oneof: Pd, Ti, Ni, Li, Au, Ag, and U; pressurizing a chamber containing thenanoparticles with one or more isotopes of hydrogen gas to load thenanoparticles with a predetermined density of hydrogen clustering; anddepressurizing the chamber to induce a reaction in the chamber. Featuresof this aspect may include the nanoparticles being a palladium richalloy and the one or more isotopes include deuterium (D₂); and thenanoparticles being a nickel rich alloy and the one or more isotopesinclude hydrogen (H₂). Further features may include forming at least onenanoscale void in the multiple of nanoparticles where forming the atleast one nanoscale void may include forming one or more of a void, achannel, a pore, a hole, and an interstitial space.

As used herein, the term “nanoscale” refers to a dimension of 100nanometers or less, and the term “microscale” refers to a dimension of100 micrometers or less. As used herein, the term “nanoparticle” refersto a solid material at standard temperature and pressure that has amaximums in two dimensions (such as width and depth) equal to or lessthan 100 nanometers, and a maximum in a third dimension (such as length)that may or may not exceed 100 nanometers. The term “metallic” refers toany composition comprising a metal atom, including but not limited to asubstance comprised multiple atoms of the same metal, alloys of two ormore different metal atoms, oxides of a metal, salts of a metal,organometallic compounds, and the like.

EXPERIMENTAL OBSERVATIONS

The following experimental observations are intended to enhance clarityand understanding of the inventive aspects of the present applicationand are not meant to be restrictive in character.

Studies have been performed in which hydrogen isotopes (¹H, deuterium (Dor ²H), and/or tritium (T or ³H)) have been loaded into thin-filmelectrodes comprised of selected metals such as palladium (Pd), titanium(Ti), and nickel (Ni). These studies indicate creation of dislocationcores in the metallic lattice that are capable of fostering hydrogencluster formation of the type indicated in FIG. 2. Evidence of suchformation includes: localized low energy nuclear reaction productsobserved in electrodes after thin film electrolysis, localized energeticcharged particle tracks in CR-39 detectors located on surface ofelectrodes during thin-film electrolysis, X-ray “beam-let” formationfrom localized sites during pulsed plasma bombardment of thin filmelectrode targets, high biding energy between hydrogen and hostmaterials verified by temperature programmed desorption experiment, andelectromagnetic SQUID and three point conductivity measurements of typeII superconductivity below 70° K in dislocation sites. Because thedensity of hydrogen or hydrogen isotopes in these sites approaches thatof metallic hydrogen, they are termed “clusters” and can be viewedconceptually as in FIG. 2. Consequently, because the atom spacing inthese clusters is so small, very little added energy or momentum isrequired to cause them to overcome the Columbic repulsion barrier andreact. As discussed here, one method to induce reactions is throughmomentum transfer to the cluster by diffusing ions (i.e., an ion fluxinto the cluster).

More specifically, a variety of thin film electrode electrolysisexperiments demonstrate local reaction sites. Early studies used amultilayer thin-film electrode with alternating layers of materials suchas Pd and Ni that have a Fermi energy level difference such as to causea high electron density (termed the “swimming electron layer”) at theinterface between thin films. Later studies used either thin filmscoated on micro-sized plastic beads or a unique thin-film cathode-anodecombination coated onto a substrate (typically a silica or ceramicsheet). In this configuration, the electric field during electrolysis isparallel to the substrate, hence along the surface direction of the thinfilms. This electric field causes a hydrogen isotope ion flow (or“flux”) in addition to the loading, thus enhancing a reaction bycollisional momentum transfer to cluster atoms. It is observed frombroad area Secondary Ion Mass Spectrometry (SIMS) analysis of theseelectrodes that the reaction products tend to occur in localized areasdistributed across the electrode. In addition, localized areas ofheating have been observed. Both the localization of products and thehot spot damage areas are indicative that reactions take place atmicro-sized sites.

CR-39 is a well known method for detection of energetic chargedparticles. CR-39 is a plastic which is damaged by passage of a chargedparticle. Subsequent etching in a NaOH solution exposes a visible trackunder a reasonable resolution microscope. Measurement of the diameterand length of the track using a microscope then gives definitive dataabout the particle involved. CR-39 detectors were placed next to thinfilm electrodes during electrolysis. CR-39 detectors (manufactured by“Landauer Co.”) rad-track chips; S=2.0×1.0 cm² were attached to Pd/Nithin film cathode; to the substrate side and/or immersed in electrolytein the cell near the electrode. The detectors were annealed to have alow initial Background before electrolysis: N(Bg)<40 track/cm². Some ofthe CR-39 was covered with a 25 μm Cu-film to identify the type ofemitted particle by its ability to penetrate this film. Several tracksfrom the CR-39 film after etching were observed. Analysis of the tracksizes correspond to 1.7 MeV protons and 14.7 MeV alpha particles. Suchparticles originate from nuclear reactions where chemical or otherphenomena cannot produce such energetic (MeV) particles.

Various plasma discharge experiments were performed in which a deuteriumgas based discharge bombards a thin-film Palladium target (cathode) in apulsed plasma discharge. Anomalous soft x-ray emission from the targetis observed which is attributed to formation of an ion cluster typeformation in the target during the pulsed loading. An experimental GlowDischarge (GD) setup was used for these studies. A positive voltage isapplied at the anode. The cathode and vessel were grounded. Plasma isproduced between this and the water-cooled cathode. The cathode ismounted on a movable mount to vary electrode spacing while the GD plasmaregion is surrounded by a glass cylinder to prevent arcing. An AXUVphotodiode detector used for x-ray detection employed a thin Be filterto block visible light from the detector. This filter cuts offx-rays<600-eV. A typical result from this detector indicates peak X-rayemission at p=500 mTorr V=250V I=2 A for a thin film Pd cathode. Thedelay time on the order of ˜msec before onset of x-rays is associatedwith D diffusion time into the target starting at the beginning of thepulsed discharge. Due to the filter X-rays are >600 eV while thedischarge voltage is 250 V. This suggests x-ray generation is due tocollective effects occurring in the cluster where the x-rays originate.A reference experiment where a thin copper foil was placed in front ofthe Be filter causes the trailing spike (i.e. the x-rays) to disappear,which confirms that the x-ray signal is not due to extraneous noisepick-up. Further supporting evidence that x-ray emission is fromlocalized sites comes from related experiments by A. Karabut, who placeda plastic “window” in the path of the x-ray beam and observed a damagepattern having numerous small isolated spots. In summary, these x-raystudies support the existence of reactive clusters in a metal targetsuch as Pd using a plasma bombardment of thin electrodes. In this case,the pulsed bombardment causes a strong inward hydrogen isotope transportwhich can stress the metal causing dislocation void formation which inturn provides the site for cluster formation. In this sense, pulsedplasma loading of hydrogen is an alternate technique to electrolyticloading described earlier.

The superconductivity of cluster-type states formed in dislocation sitesin Pd has been studied. These experiments used a special cyclic“loading-deloading” technique to create stress-induced dislocation sitesfostering cluster formation. Two separate techniques were used in thestudy: (1) H₂ gas pressure loading-deloading cycles were applied to asingle crystal thin film Pd electrode with the deloading taking placefor 2 hours. Alternately, electrochemical cycling (cathodeloading-anodic deloading) with a current of 5.0 mA/cm² in 1M Li₂SO₄/H₂Owas used with a Pd/PdO cold-worked electrode. Both electrodes wereinitially prepared by annealing for 2 hours at about 580 K. Theelectrodes were subsequently examined for ferromagnetic propertiesassociated with superconductivity using a “Quantum Design” 1T-SQUID typeinstrument operating in either DC or AC modes. The results from theSQUID measurements are summarized as follows. After repeated H-cycling,both the Pd:H_(x) and Pd/PdO:H_(x) samples contained an ultra-highdensity condensed hydrogen phase inside the dislocation sites or “cores”(void regions). While the average loading ratio (atoms H/Pd) of theelectrodes was only (3.8−5.5)×10⁻⁴ with respect to the gross samplevolume, local loading ratios (defined as the rates of H or D toimmediately surrounding Pd lattice atoms) as high as ˜5-1000 occurredinside the clusters formed in the small dislocation cores. The loadingratio in the cluster region depends on the core size relative to thelattice spacing. In the present case loading ratios varied over a largerange due to a random distribution of core sizes. The SQUID measurementsof the electrodes demonstrated a weak type II superconductivity,involving a condensed hydrogen phase in the dislocation sites (i.e.“cores”) below ˜30 Kelvin (K). Both magnetic and transport measurementsof the electrodes indicate a superconducting transition below ˜70 K. Areproducible Meissner-effect was obtained in 1 kHz AC field at H≦1.0 Oe.In summary, these results show that the localized clusters are in acondensed mode giving metallic-like properties with low temperaturesuperconductivity properties in the H-loaded dislocation corescorresponding to hydrogen clusters.

The hydrogen clusters formed in the H-loaded dislocation sites arestable unless a triggering technique occurs which causes a diffusinghydrogen or deuterium ion to enter the cluster region and transfermomentum to a cluster atom. Subsequent reactions can be appropriatelydescribed as pyconuclear reaction theory. Pyconuclear reactions inastrophysical objects address behavior of a high density of hydrogenisotopes, and correspondingly provide a basis for considering hydrogencluster behavior in dislocation cores, because the atom density in theseclusters is similar. Such reactions are believed to take place even at“zero temperature” in condensed matter due to ions fluctuating abouttheir lattice sites in coherence with the zero-point energy, E₀≈hω_(o).The addition of momentum by the “triggering” event already noted can beviewed as elevating the “temperatures” as subsequent collisions equalizethe added fluctuations over the cluster atoms. Due to close spacing andthis fluctuation, these ions may penetrate the Coulomb barrier of aneighboring ion causing nuclear reactions provided there is a sufficientflux of ions to transfer momentum to the stationary cluster atoms.

In hydrogen-loaded dislocation cores or nanoparticle structures, clusteror ions have a close spacing and a higher fluctuation frequency becausethey have a finite temperature. Pyconuclear principles can be appliedwith a temperature (fluctuation frequency) correction. Further,hydrogen-loaded cluster or particle behavior is also enhanced by thestrong diffusion (sometimes called “hopping”) of the hydrogen isotope(such as H or D) during loading (or deloading). The diffusing ions flowthrough the cluster or ion sites, undergoing collisions with the clusteror ion atoms, thus transmitting momentum to them. This enhances theoscillations of the cluster or ion atoms and can be roughly account forthe added collisional energy. Calculations based on this theory, showthat the higher reaction rates such as observed in the low energyreaction experiments correspond to this flow. The electrolytic thin-filmexperiments have a relatively high flow of “flux” correction due to thedesign of the electrodes in FIG. 1 a creating a driving electric field.The low rate radiation emission experiments have a much lower flowcorrection while superconducting structures do not involve flow.

Reaction rate calculations without flow based on conventionalPyconuclear reaction theory are presented as follows along withcalculations where the flow is included through use of an effectivetemperature. Now turn to reactions in a crystal lattice or interstitialspacing. The reaction rate per ion pair is

$\begin{matrix}{W = {\left( {{inc}.{flux}} \right) \times T \times 4\;{\pi R}_{n}^{2}P_{n}}} \\{= {v{\psi_{inc}}^{2}\frac{{TS}(E)}{E}}}\end{matrix}$where we have to caculate |ψ_(inc)|² and T using the lattice potentialfor r>R_(n). The measured nuclear factor S(E) remains the same asbefore.

${P_{0} = {\left( \frac{\rho}{A} \right)A^{2}Z^{4}S_{\gamma}\lambda^{7/4}{\exp\left( {{- ɛ}\;\lambda^{{- 1}/2}} \right)}s^{- 1}{cm}^{- 3}}},{with}$γ = 3.90 × 10⁴⁶, ɛ = 2.638.

Results using these calculations confirm that the reaction rate stronglydepends on dislocation core or inter-particle loading and on flow rate.For example, in the cyclic loading-deloading a low rate of chargeparticle emission was seen from CR-39. Much higher reaction rates wereobtained in thin film reactions. The cluster or ion loading (atoms ofD/atoms Pd) along with the flow rate were varied in calculations tomatch the experimentally observed reaction rates (rx/cm3-sec): (a) forlow rates of ˜1 reaction/cm³-sec, as in the CR-39 tracks duringunloading (flow), a local loading of ˜8 D/Pd matches without flow andfor flow matching of the deloading value, only ˜2 D/Pd are required; and(b) for high reaction rates, e.g. 10¹⁴ reactions/cc-s, a local loadingof ˜12 D/Pd matches with an estimated flow 5× the deloading value usedabove. Consequently, developments in pyconuclear astrophysics areconsistent with hydrogen cluster or ion behavior in dislocation orinter-particle sites. Because of its nonlinearity, it is expected thatthe predicted reaction rate increases rapidly with higher hydrogenisotope loading and flow rate. Further, with little or no flow rate, aviable superconducting state results in correspondence to the degree ofloading.

Many further embodiments of the present application are envisioned. Forexample, one further embodiment comprises: establishing a predefinedtarget representative of a desired dislocation core density of amultilayer thin film device design; forming a multilayer thin filmdevice according to the design; and after forming it, loading themultilayer thin film device with an amount of one or more isotopes ofhydrogen to form hydrogen clusters in the dislocation cores. In oneform, the formation of the multilayer thin film device includesproviding a first layer of a first type of metal and a second layer of asecond type of metal dissimilar from the first type of metal, andpreparing an interface between the first layer and the second layer toincrease a quantity of the dislocation cores there along and incorrespondence with the predefined target.

Another example includes preparing a multilayer thin film deviceincluding a first layer of a first type of metal and a second layer of asecond type of metal dissimilar from the first type of metal;repetitively loading it and deloading the device with one or moreisotopes of hydrogen at least ten times during the preparing thereof;and supplying a flow of at least one isotope of hydrogen to operate thedevice.

Still another example comprises: a multilayer thin film device includinga first layer of a first type of metal and a second layer of a secondtype of metal dissimilar from the first type of metal, means forrepetitively loading and deloading the device with one or more isotopesof hydrogen during the preparation thereof, and means for supplying aflow of at least one isotope of hydrogen to the device.

Yet another embodiment comprises: preparing a multilayer thin filmdevice including a first layer of a first type of metal and a secondlayer of a second type of metal dissimilar from the first type of metal;providing nanoscale voids along an interface between the first layer andthe second layer during the preparing of the multilayer thin filmdevice, which includes at least one of (a) placing nanoscale materialalong the interface and (b) forming one or more of a plurality ofchannels, pores, holes, or voids in one or more of the first layer andthe second layer, and supplying one or more isotopes of hydrogen to thedevice to form hydrogen clusters therein.

A further example includes: a source of one or more isotopes ofhydrogen, a multilayer thin film device in communication with the sourceto receive the one or more isotopes of hydrogen therefrom, themultilayer thin film device including a first layer and a second layerof a different material than the first layer, the first layer being of ametallic type effective to form a hydride with the one or more isotopesof hydrogen, an interface between the first layer and the second layerand a material positioned along the interface to form a plurality ofnanoscale voids to increase a quantity of dislocation cores formed alongthe interface and correspondingly increases loading of the one or moreisotopes of hydrogen from the source. In one form, the material includesone or more of micro-scale particles, fibers, wires, and mesh.Alternatively or additionally, the material includes a porous metallicsubstance.

Still a further embodiment comprises a multilayer thin film deviceincluding a first layer with means for forming a hydride with one ormore isotopes of hydrogen and a second layer of a material differentthan the first layer; means for increasing dislocation core formationalong an interface between the first layer and the second layer; andmeans for supplying the multilayer thin film device with at least oneisotope of hydrogen.

Any theory, mechanism of operation, proof, or finding stated herein ismeant to further enhance understanding of the present invention and isnot intended to make the present invention in any way dependent uponsuch theory, mechanism of operation, proof, or finding. It should beunderstood that while the use of the word preferable, preferably orpreferred in the description above indicates that the feature sodescribed may be more desirable, it nonetheless may not be necessary andembodiments lacking the same may be contemplated as within the scope ofthe invention, that scope being defined by the claims that follow. Inreading the claims it is intended that when words such as “a,” “an,” “atleast one,” “at least a portion” are used there is no intention to limitthe claim to only one item unless specifically stated to the contrary inthe claim. Further, when the language “at least a portion” and/or “aportion” is used the item may include a portion and/or the entire itemunless specifically stated to the contrary. The present applicationhereby incorporates by reference all publications, patents and patentapplications set forth herein, including but not limited to: G. H.Miley, and J. A. Patterson, “Nuclear Transmutation in Thin-film CoatingsUndergoing Electrolysis,” Journal New Energy, Vol. 1, pp. 11-15 (1993);G. H. Miley, G. Name, T. Woo, “Use of Combined NAA and SIMS Analyses forImpurity Level Isotope Detection,” Journal of Radioanalytical andNuclear Chemistry, Vol. 263, No.3, pp. 691-696 (2005); G. H. Miley andP. J. Shrestha, “Review of Transmutation Reactions in Solids,” CondensedMatter Nuclear Science, P. Hagelstein and S. Chubb, eds., WorldScientific Press, New Jersey, pp. 364-378 (2006); A. G. Lipson, G. H.Miley, A. S. Roussetski, and E. I. Saunin, “Phenomenon of EnergeticCharged Particle Emission from the Hydrogen/Deuterium Loaded Metals,”Condensed Matter Nuclear Science, P. Hagelstein and S. Chubb eds., WorldScientific Press, New Jersey, pp. 539-575 (2006); G. H. Miley and A. G.Lipson, “Intense X-ray Emission from Highly Loaded Hydrides,” Proc. ofSPIE, Vol. 5197, p. 35 (2004); A. Lipson, G. H. Miley, et al.,“Emergence of a High-Temperature Superconductivity in Hydrogen Cycled PdCompounds Suggest Localized Superstochiometric H/D Sites,” Proceedings,ICCF-12, Nagoya, Japan (2005); Lipson, B. Heuser, C. Castano, G. Miley,B. Lyakhov, and A. Mitin, “Transport and Magnetic Anomalies below 70 Kin a Hydrogen-cycled Pd Foil with a Thermally Grown Oxide,” PhysicalReview, B 72, 212507, Dec. 13 (2005); S. Ichimaru and H Kitamura,“Pyconuclear Reactions in Dense Astrophysical and Fusion Plasmas,” Phys.Plasmas, Vol. 6, No. 7, pp. 2649-2671 (1999); X. Yang, G. H. Miley, K.A. Flippo, S. A. Gaillard, D. T. Offermann, H. Hora, B. B. Gall, T.Burris-Mog, J. Rassuchine, C. Plechaty, J. Ren, “D-Cluster ConverterFoil for Laser-Accelerated Deuteron Beams: Towards Deuteron-Beam-DrivenFast Ignition,” Fusion Science and Technology, Vol. 60, No. 2, pp.615-619 (2011); Y. E. Kim, “Theory of Bose-Einstein CondensationMechanism for Deuteron-Induced Nuclear Reactions in Micro/Nano-ScaleMetal Grains and Particles,” Naturwissenschaften, Vol. 96, pp. 803-811(2009). While the invention has been illustrated and described in detailin the drawings and foregoing description, the same is to be consideredas illustrative and not restrictive in character, it being understoodthat only the selected embodiments have been shown and described andthat all changes, modifications and equivalents that come within thespirit of the invention as defined herein or by any of the followingclaims are desired to be protected.

What is claimed is:
 1. A method comprising: operating a gas loadingsystem including: a source of one or more isotopes of hydrogen, a gasloading chamber containing a number of metallic nanoparticles, thenanoparticles being selected to provide for a predetermined hydrogencluster formation density, a vacuum system, and a valve system incommunication with the gas loading chamber, the source of one or moreisotopes of hydrogen and the vacuum system; providing the gas loadingchamber with a first quantity of the one or more isotopes of hydrogenfrom the source of one or more isotopes of hydrogen; monitoring anoperating temperature; and cycling a loading pressure of the gas loadingchamber using the source of one or more isotopes of hydrogen in responseto providing the gas loading chamber and monitoring the operatingtemperature.
 2. The method of claim 1, which includes reloading thechamber with a second quantity of the one or more isotopes of hydrogenfrom the source.
 3. The method of claim 1, wherein the metallicnanoparticles include a palladium rich alloy and the first quantity ofthe one or more isotopes of hydrogen includes deuterium (D₂).
 4. Themethod of claim 3, wherein the palladium rich alloy further includesabout 35 weight percent palladium and about 65 weight percent zirconium.5. The method of claim 1, wherein the metallic nanoparticles include anickel rich alloy to produce a quantity of nanoparticles and the firstquantity of the one or more isotopes of hydrogen further includeshydrogen (H₂).
 6. The method of claim 5, wherein the nickel rich alloyfurther includes about 20 to about 35 weight percent palladium, about 15weight percent nickel and about 50 to about 65 weight percent zirconium.7. The method of claim 1, which further includes providing a thermalmanagement system.
 8. The method of claim 7, wherein providing thethermal management system further includes providing at least one of aheating element and a cooling element.
 9. The method of claim 7, furtherincluding: removing impurities with a vacuum in the gas loading chambercontaining the number of metallic nanoparticles; and desorbing aquantity of gases by heating the gas loading chamber containing thenumber of metallic nanoparticles.
 10. A system comprising: a gas sourceto provide one or more isotopes of hydrogen; a plurality of metallicnanoparticles; a chamber containing the metallic nanoparticles andstructured to receive the one or more isotopes of hydrogen from the gassource; a vacuum system; and a valve system in communication with thechamber, the gas source and the vacuum system; wherein the valve systemis capable of directing a first quantity of the one or more isotopes ofhydrogen from the gas source into the chamber under a gas loadingpressure provided by the vacuum system and directing a second quantityof the one or more isotopes of hydrogen from the chamber therebyreducing the gas loading pressure.
 11. The system of claim 10, whereinthe valve system is further capable of directing a third quantity of theone or more isotopes of hydrogen from the gas source into the chamberunder a second gas loading pressure provided by the vacuum system. 12.The system of claim 10, wherein the valve system further includes afirst valve to disconnect the vacuum system from the gas loading chamberand a second valve to disconnect the hydrogen gas source from the gasloading chamber.
 13. The system of claim 10, wherein the nanoparticlesinclude a palladium alloy and the first quantity of hydrogen includesdeuterium (D₂).
 14. The system of claim 13, wherein the palladium alloyfurther includes about 35 weight percent palladium and about 65 weightpercent zirconium.
 15. The system of claim 10, wherein the nanoparticlesinclude a nickel alloy and the first quantity of hydrogen includeshydrogen (H₂).
 16. The system of claim 15, wherein the nickel alloyfurther includes about 20 to about 35 weight percent palladium, about 15weight percent nickel and about 50 to about 65 weight percent zirconium.17. The system of claim 10, which further includes a thermal managementsystem.
 18. The system of claim 17, wherein the thermal managementsystem further includes at least one of a heating element and a coolingelement.
 19. The system of claim 17, which further includes directing aquantity of initial gases from the chamber containing the nanoparticleswherein the thermal management system is capable of modifying atemperature of the chamber containing the nanoparticles during directingthe quantity of initial gases.
 20. A method, comprising: providingseveral nanoparticles each comprised of at least one of: Pd, Ti, Ni, Li,Au, Ag, and U; pressurizing a chamber containing the nanoparticles withone or more isotopes of hydrogen gas to load the nanoparticles with apredetermined density of hydrogen clustering; and depressurizing thechamber to induce a reaction in the chamber.
 21. The method of claim 20,wherein the nanoparticles further include a palladium rich alloy and theone or more isotopes include deuterium (D₂).
 22. The method of claim 20,wherein the nanoparticles further include a nickel rich alloy and theone or more isotopes include hydrogen (H₂).
 23. The method of claim 20,further includes forming at least one nanoscale void in the multiple ofnanoparticles.
 24. The method of claim 23, wherein forming the at leastone nanoscale void includes forming one or more of a void, a channel, apore, a hole, and an interstitial space.